Determination of gold, platinum and palladium in geological samples by inductively coupled plasma-mass spectrometry after separation and preconcentration with C-410 anion exchange resin

A method for the determination of Au, Pt and Pd in geological samples is described. Au, Pt and Pd can be separated and concentrated quantitatively by C-410 anion-exchange resin in the condition of 1.5 mol/L HCl with the adsorption rates of 91.2%, 100.0% and 95.7% respectively. No interference exists from coexisting elements except for Ge(IV), Cr(VI),Ti(IV) in inductively coupled plasma-mass spectrometry. The detection limits are 0.27 mug/L, 0.40 mug/L and 0.19 mug/L for Au, Pt and Pd respectively. The results of these elements in standard geological materials are in agreement with certified values with precision of 19.2% RSD for Au (n = 8), 28.1% RSD for Pt (n=8), and 15.6% RSD for Pd (n=8).

Separation of heavy rare earth elements with extraction resin containing 1-hexyl-4-ethyloctyl isopropylphosphonic acid

This paper presents the results of the adsorption of heavy rare earth ions (Gd(III), Tb(III), Dy(III), Ho(III), Er(III), Tm(III), Yb(III), Lu(III) and Y(III)) from hydrochloric acid solutions at 30 degreesC by the extraction resin containing 1-hexyl-4-ethyloctyl isopropylphosphonic acid (HEOPPA), which has higher steric hindrance, higher selectivities and lower extraction and stripping acidity than di(2-ethylhexyl)phosphoric acid (DERPA) or 2-ethylhexyl phosphonic acid mono-2-ethylhexyl ester (HEH/EHP). The dependence of acid concentration, flow rate and amounts of rare earth ions sorbed on the separation of Er-Tm, Tm-Yb and Er-Tm-Yb mixtures has been studied. The baseline chromatographic separation of Er-Tm-Yb mixture has been observed. Satisfactory results with purity and yield of Tm2O3>99.71% and >71.25%, Er2O3>99-81% and >94.17%, and Yb2O3>99.74% and >89.83%, respectively, have been obtained. The parameters such,as resolution, separation factors and efficiencies have been determined as a function of acidity, loading of rare earth elements and flow rates. The stoichiometry of the extraction of rare earth ions has been suggested as well.

The preparation of phenolic resin/montmorillonite nanocomposites by suspension condensation polymerization and their morphology

Phenolic resin/clay nanocomposites were prepared using a suspension condensation polymerization method that was suitable to both novolac and resole. Natural montmorillonite and two kinds of organic modified montmorillonite were adopted to investigate the effect of modification on the final morphology of the nanocomposites. X-ray diffraction (XRD) measurements and Transmission Electron Microscope (TEM) observations showed that clay platelets were easier to be exfoliated or intercalated in novolac than in resole because novolac usually has a linear structure. The modifier with a phenyl ring was more compatible with novolac (or resole) than the aliphatic type modifier. The influence of curing on the morphology was studied as well. An exfoliation-adsorption and in situ condensation mechanism was proposed on the formation of the nanocomposites.

Liquid-phase hydrogenation of furfural to tetrahydrofurfuryl alcohol catalyzed by polymer resin supported palladium catalysts

Three kinds of polymer resin supported Pd catalysts were prepared by mixing PdCl2, with alkaline styrene anion exchange resins[D392 -NH2, D382, -NHCH3, D301R, -NH(CH3)(2)], strongly alkaline styrene anion exchanged resin [201 X 7DVB, -NH+ (CH3)(3)] and alkaline epoxy exchange resin (701, -NH2), and hydrogenating in liquid phase at 1.013 X 10(5) Pa. The hydrogenation of furfural was studied under the reaction conditions such as solvent, temperature. Pd content in the supported catalyst and the amount of the catalyst. The yield of hydrogenation reaction of furfural markedly increased to 100% and the selectivity to tetrahydrofurfuryl alcohol increased to over 98% by polymer (alkaline styrene anion exchange resins D392, -NH2, D382, -NHCH3) supported palladium catalysts comparing with the yield over 70% and selectivity over 97% by palladium catalyst, in 50% alcohol-50% water or pure water solution at 1.013 X 10(5) Pa. The relationship between hydrogenation and the structures of functional group in the supporting resin was examined by XPS method.

Preparation and characterization of phenoxy resin/poly(4-vinylpyridine) interpolymer complexes

The compositions and structures of interpolymer complexes formed by mixing phenoxy resin (PHEB) and poly (4-vinylpyridine) (P4VPy) in chloroform have been studied by means of elemental analysis, DSC, FTIR, UV and XPS, In the meantime, the corresponding blends prepared have been characterized and compared. The results show that compositions of the complexes were identical with the ratio of equimolar interactive units. All blends were miscible and their compositions were related to the feed ratios. Based on the experimental results, process of formation of the complex is depicted.

Extraction and separation of heavy rare earth (III) with Extraction Resin containing di(2,4,4-trimethyl pentyl) phosphinic acid (Cyanex 272)

Extraction resins, of the type of;levextrel, (which is a collective term for styrene/divinylbenzene based copolymers of predominantly macroporous structure that contain a selective extractant) are important for the recovery and separation of metal ions, as they combine features of solvent extraction and ion exchange resins. This paper presents the results of the adsorption of heavy rare earth ions (Ho(III), Er(III), Tm(III), Yb(III), Lu(III) and Y(III)) from hydrochloric acid solutions at 0.2 mol/L ionic strength and 50 degrees C by the extraction resin containing di (2,4,4-trimethyl pentyl) phosphinic acid (Cyanex 272) and the chromatographic separation of (Er(III), Tm(III) and Yb(III)). Technological separation products, with purity and yield of Tm2O3 >99.97%, >80%, Er2O3 >99.9%, >94% and Yb2O3 >99.8%, >80% respectively, have been obtained from a feed having the composition Tm2O3 60%, Er2O3 10%, and Yb2O3 3%, the others 27%. The distribution coefficients, extraction equilibrium constants and separation factors have been determined as a function of acidity, loading of the resin and rare earths, flow rates and column ratios. The resolutions and efficiencies of separation of Er/Tm/Yb each other have been calculated. The stoichiometry of the extraction of rare earth ions has been suggested as well.

Use of SAXS to characterize the morphology of poly(polyethylene glycol diacrylate)/epoxy resin interpenetrating networks

Interpenetrating polymer networks (IPNs) have been synthesized from prepolymers that form miscible blends. All IPNs made from polyacrylate ((polyethylene glycol diacrylate), PEGDA) and epoxy (diglycidyl ether of bisphenol A, DGEBA) can be made in phase separated states by incorporating crosslinks. However, blends of these prepolymers, having a negative Flory-Huggins interaction parameter, are highly miscible. This indicates that formation of IPNs favours phase separation relative to blends. The microphase separation characteristics in the PEGDA/DGEBA IPNs were determined using smalt-angle X-ray scattering (SAXS). The Debye-Bueche and Guinier methods were used to calculate the correlation lengths of the segregated phases existing in the PEGDA/DGEBA IPNs. The results from SAXS showed that the size of the phase segregation zones changed with composition from about 50 to 100 Angstrom.

SYNTHESIS AND ORIENTATION OF MELAMINEALDEHYDE RESIN CROSS-LINKED POLYMERS

Three kinds of hydroxy-terminated oligomers were synthesized and characterized by IR, DSC and GPC. The oligomers were crosslinked by melaminealdehyde resin. The orientation and relaxation of the poled and crosslinked polymers were studied by UV-Vis spectra. It was shown that polymers had high orientational stability after corona-poling and crosslinking.

THE RADIATION STABILITY OF PERFLUOROALKOXY RESIN

By examining the changes in melting temperature, heat of fusion, tensile strength and ultimate elongation at 150-degrees-C, and weight loss, radiation effects on perfluoroalkoxy resins (PFA) were investigated. The results show that at the temperatures used here the predominant effect caused by radiation on PFA is degradation of the molecular weight. The radiation stability is much better than that of polytetrafluoroethylene, however.

PHASE-BEHAVIOR IN EPOXY-RESIN CONTAINING PHENOLPHTHALEIN POLY(ETHER ETHER SULFONE)

Phenolphthalein poly(ether ether sulphone) (PES-C) was found to be miscible with uncured bisphenol-A-type epoxy resin, i.e. diglycidyl ether of bisphenol A (DGEBA), as shown by the existence of a single glass transition temperature within the whole composition range. Miscibility between PES-C and DGEBA is considered to be due mainly to the entropy contribution. However, dynamic mechanical analysis (d.m.a.) and scanning electron microscopy (SEM) studies revealed that PES-C exhibits different miscibility with four cured epoxy resins (ER). The overall compatibility and the resulting morphology of the cured blends are dependent on the choice of cure agent. For the blends cured with amines (4,4'-diaminodiphenylmethane (DDM) and 4,4'-diaminodiphenylsulphone (DDS)), no phase separation occurs as indicated by either d.m.a. or SEM. However, for the blends cured with anhydrides (maleic anhydride (MA) and phthalic anhydride (PA)), both d.m.a. and SEM clearly show evidence of phase separation. SEM study shows that the two phases interact well in the MA-cured blend while the interface between the phases in the PA-cured blend is poorly bonded. The differences in the overall compatibility and the resulting morphology between the amine-cured and anhydride-cured systems have been discussed from the points of view of both thermodynamics and kinetics.

PHASE-SEPARATION IN ANHYDRIDE-CURED EPOXY-RESIN CONTAINING PHENOLPHTHALEIN POLY(ETHER ETHER KETONE)

Dynamic mechanical analysis and scanning electron microscopy were used to study phase separation of three blends of anhydride-cure bisphenol-A-type epoxy resin with phenolphthalein poly(ether ether ketone). Phase separation was observed for all the blends. The overall compatibility and the resulting morphology of the cured blends are dependent on the choice of cure agent. The phenomena have been discussed from the points of view of both thermodynamics and kinetics. The effects of the choice of hardener on phase separation are considered to be primarily due to differences between the chemical natures of the hardeners.

THE MISCIBILITY AND MORPHOLOGY OF EPOXY-RESIN POLY(ETHYLENE OXIDE) BLENDS

Poly(ethylene oxide) (PEO) was found to be miscible with uncured epoxy resin, diglycidyl ether of bisphenol A (DGEBA), as shown by the existence of a single glass transition temperature (T(g)) in each blend. However, PEO with M(n) = 20 000 was judged to be immiscible with the highly amine-crosslinked epoxy resin (ER). The miscibility and morphology of the ER/PEO blends was remarkably affected by crosslinking. It was observed that phase separation in the ER/PEO blends occurred as the crosslinking progressed. This is considered to be due to the dramatic change in the chemical and physical nature of ER during the crosslinking.

BLENDS OF PHENOLPHTHALEIN POLY(ETHER ETHER KETONE) WITH PHENOXY AND EPOXY-RESIN

The properties of miscible phenolphthalein poly(ether ether ketone)/phenoxy (PEK-C/phenoxy) blends have been measured by dynamic mechanical analysis and tensile testing. The blends were found to have single glass transition temperatures (T(g)) that vary continuously with composition. The tensile moduli exhibit positive deviations from simple additivity. Marked positive deviations were also observed for tensile strength. The tensile strengths of the 90/10 and 75/25 PEK-C/phenoxy blends are higher than those of both the pure components. Embrittlement, or transition from the brittle to the ductile mode of failure, occurs in the composition range of 50-25 wt% PEK-C. These observations suggest that mixing on the segmental level has occurred and that there is enough interaction between the components to decrease its internal mobility significantly. PEK-C was also found to be miscible with the epoxy monomer, diglycidyl ether of bisphenol A (DGEBA), as shown by the existence of a single glass transition temperature (T(g)) within the whole composition range. Miscibility between PEK-C and DGEBA could be considered to be due mainly to entropy. However, PEK-C was judged to be immiscible with the diaminodiphenylmethane-curved epoxy resin (DDM-cured ER). It was observed that the PEK-C/ER blends have two T(g), which remain invariant with composition and are almost the same as those of the pure components, respectively. Scanning electron microscopy showed that the PEK-C/ER blends have a two-phase structure. The different miscibility with PEK-C between DGEBA and the DDM-cured ER is considered to be due to the dramatic change in the chemical and physical nature of ER after curing.

Recovery of silver (I) using a thiourea-modified chitosan resin

This work describes the preparation of a chelating resin from chemically modified chitosan. The resin was synthesized by using O-carboxymethylated chitosan to cross-link a polymeric Schiffs base of thiourea/glutaraldehyde and characterized by IR. Batch method was applied for testing the resin's adsorption behavior. Adsorption experiments showed the resin had good adsorption capacity and high selectivity for Ag(I) in aqueous solution. The maximum uptake of Ag(I) exhibited was 3.77 mmol/g, at pH 4.0. The results also indicated that the adsorption process was exothermic and fit well with the pseudosecond-order kinetic model. Ag(I) desorption could reach 99.23% using 0.5 M thiourea-2.0 M HCl solution. (C) 2010 Elsevier B.V. All rights reserved.